ABSTRACT The distorted octahedral oxorhenium(V) complex [ReOCl(had)] (1) (H2had = N,N-bis(2-hydroxybenzyl)-2-(2-aminoethyl)dimethylamine) was prepared from the oxidation of [ReCl3 (MeCN)(PPh3)2] by dioxygen in the presence of H2 had in ethanol. This reaction was done under reflux conditions for a relatively short reaction time of an hour. However, increasing the reaction period to seven days led to the disproportionation of 1 to [ReIVCl(had)(PPh3)](Re sup>VIIO4) (2). Both compounds were characterized by infra-red spectroscopy and X-ray crystallography.